CN105483376B - A kind of high-cobalt zinc sulfate solution removes cobalt agent and its Technology for removing cobalt - Google Patents
A kind of high-cobalt zinc sulfate solution removes cobalt agent and its Technology for removing cobalt Download PDFInfo
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- CN105483376B CN105483376B CN201510932637.9A CN201510932637A CN105483376B CN 105483376 B CN105483376 B CN 105483376B CN 201510932637 A CN201510932637 A CN 201510932637A CN 105483376 B CN105483376 B CN 105483376B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
- C22B3/46—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes by substitution, e.g. by cementation
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- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
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Abstract
Cobalt agent and its Technology for removing cobalt are removed the invention discloses a kind of high-cobalt zinc sulfate solution, belongs to Purification of zinc sulfate solution production technical field.It include filtering, system one it is quiet after liquid, system two it is quiet after liquid, prepare except cobalt agent A, prepare except cobalt agent B, two it is quiet after liquid preheating, mix, press filtration, obtain new liquid, except cobalt agent be except cobalt agent A with except cobalt agent B mixture.The present invention can thoroughly solve the problem of zinc powder excess during Purification of zinc sulfate solution, not only reduce the usage amount of zinc powder, improve the utilization rate of zinc powder, while also improve the stability of Purification of zinc sulfate solution quality.
Description
Technical field
It is molten more specifically to a kind of high-cobalt zinc sulfate the invention belongs to Purification of zinc sulfate solution production technical field
Liquid removes cobalt agent and its Technology for removing cobalt.
Background technology
At present, the Technology for removing cobalt of solution of zinc sulfate mainly has antimonic salt method, arsenic method, Huang in domestic and international electrolytic zinc production process
Medicine method and Beta Naphthol 99MIN method.In antimonic salt method and arsenic method technique, make the additive of purification process using arsenic or antimonic salt.Except cobalt
Principle is more electropositive in certain pH, temperature and stirring intensity similarly hereinafter solution of zinc sulfate based on more electronegative zinc powder
Cobalt ions chemically reacts, so as to which cobalt ions be cemented out from solution.Addition antimonic salt or arsenic are exactly to reduce cobalt
The ultra-voltage of ion, so as to improve the thermodynamic condition of its displacement, realize effective removing of cobalt ions.Using arsenic as purification
Although additive detergent power is strong, zinc consumption is low, and process is also easy to produce extremely toxic substance As H3, and it is hidden to there is larger safety
Suffer from；And the former is compared, no extremely toxic substance generation low as purification additive, depletion of additive using antimonic salt, but zinc powder be present and disappear
Larger, purification process temperature requirement height is consumed, large steam consumption, the larger scattered of cobalt be present.Xanthate purification method technological work environment
Difference, operator is difficult to receive and environmental pollution is serious, and need to add the shortcomings of copper sulphate does activator and big xanthate stink
Gradually it is eliminated；Beta Naphthol 99MIN method Technology for removing cobalt flow is as follows：Middle supernatant → use one section of copper removal of zinc powder, cadmium → press filtration (it is net to obtain one
Liquid afterwards) → Beta Naphthol 99MIN except cobalt → activated carbon decolorizing → press filtration (two net after liquid) → deep copper removal, cadmium → press filtration → new liquid.Should
Process costs are high, and Beta Naphthol 99MIN and activated carbon can not recycle, serious waste of resources.
Caused purification slag does not use generally in zinc sulfate purification process, and this allows in purification slag contained
A large amount of zinc powders not reacted completely fail to be fully used, and cause the rising of processing cost, and be also unfavorable for depuration quality
Stability contorting.Due to the market factor, the continuous decline for the zinc concentrate grade that enterprise is purchased, and impurity content more and more higher.
Especially in purification process in solution cobalt impurity removing, turn into one piece of high " heart of cost in enterprise production process
Disease ".Therefore, find a kind of stable solution of zinc sulfate of depuration quality in electrolytic zinc production technology except cobalt new technology have it is important
Meaning.
The content of the invention
1st, to solve the problems, such as
For the above-mentioned problems in the prior art, the present invention provide a kind of high-cobalt zinc sulfate solution except cobalt agent and its
Technology for removing cobalt, thoroughly solve the problem of zinc powder excess during Purification of zinc sulfate solution, not only reduce the usage amount of zinc powder, carry
The high utilization rate of zinc powder, while also improve the stability of Purification of zinc sulfate solution quality.
2nd, technical scheme
In order to solve the above problems, the technical solution adopted in the present invention is as follows：
A kind of high-cobalt zinc sulfate solution removes cobalt agent and its Technology for removing cobalt, it is characterised in that comprises the following steps：
(1) at normal temperatures, supernatant solution in zinc sulfate is accurately filtered using Sean filter, after making accurate filtering
Solution solids suspension content be less than 50mg/L；
(2) by the middle supernatant solution after filtering, under the conditions of 70-80 DEG C, zincification powder 2.0-2.5Kg/m3, stirring reaction
0.5-1.0h, press filtration, obtain a net rear liquid；
(3) by one it is net after liquid temperature adjusting to 55-65 DEG C, be continuously added into zinc powder, stirring reaction 0.5-1.0h, press filtration, directly
Into solution, each primary metal ion concentration reaches finite concentration, stops adding zinc powder, obtains two net rear liquid, and determine cobalt therein
Content；
(4) add by the content of cobalt content and other metal ions in the step (3) two liquid after net to calculate glycine
Enter amount；
(5), will after the glycine that content is determined in the step (4) is dissolved with industrial water by solid-liquid=0.1-0.2
PH value is adjusted to 8.0-9.0, obtains except cobalt agent-A；
(6) natrium nitrosum is calculated by the content of cobalt content and other metal ions in the step (3) two net rear liquid
Addition；
(7) after the natrium nitrosum that content is determined in the step (6) is dissolved with industrial water by solid-liquid=0.2-0.3,
Cobalt agent-B must be removed；
(8) two net rear liquid are preheated to 55-80 DEG C；
(9) by except cobalt agent-A and except cobalt agent-B is added in two after preheating net rear liquid, 2-5min is stirred；
(10) the net rear liquor pH value of gained two in the step (9) is adjusted to 2.5-5.0, and keeps solution temperature to exist
55-80 DEG C, stirring reaction 1.0-2.0h；
(11) press filtration, obtains new liquid, and remaining concentration of cobalt ions≤0.3mg/L, other metal ions meet electrode in new liquid
It is required that.
Further, when the concentration that each primary metal ion reaches is in step (3) solution：Zn 120-150g/L,
Cd 1-50mg/L, Cu 0.01-0.3mg/L, Ni 0.1-1.5mg/L, Fe 1.0-2.0mg/L, Ge 0.01-0.02mg/L, stop
Only add zinc powder.
Further, the addition of step (3) zinc powder is between 1.0-1.5Kg/m3Between.
Further, the calculation formula of glycine addition is in the step (4)：Glycine addition (mg/L)=
{ Co concentration (mg/L)+Fe concentration (mg/L) } × (4-6)+{ other concentration of metal ions (mg/L) × (2-4) }.
Further, the calculation formula of step (6) the Sodium Nitrite addition is：Natrium nitrosum addition (mg/L)
={ Co concentration (mg/L)+Fe concentration (mg/L) } × (2-4).
Further, the material that the step (10) is used for adjusting pH value is sulfuric acid, the useless electrolysis of Zn system electrolysis output
Any of liquid, acetic acid, nitric acid, phosphoric acid.
Further, the glycine addition is by middle survey cobalt content in two net rear liquid 4-6 times of the step (3).
Further, 1-2 of the natrium nitrosum addition by surveying cobalt content in two net rear liquid in the step (3)
Times.
Further, it is described except cobalt agent is except cobalt agent-A in the step (7) with removing cobalt in the step (5)
Agent-B mixture.
3rd, beneficial effect
Compared to prior art, beneficial effects of the present invention are：
(1) present invention is by the detection to component content in solution of zinc sulfate, and keeps a record, then adjusts solution of zinc sulfate
PH value is 2.5-5.0, and then causes zinc sulfate to disclosure satisfy that condition requirement in the follow-up purifying process of progress, promotes zinc sulfate
The elimination factor of middle Zn, Cd, Cu, Ni, Fe, Ge element, improve the purity of solution of zinc sulfate；And combine processing procedure addition and remove cobalt
Agent is stirred again, then adds zinc powder thereto, is stirred for filtering so that Zn, Cd, Cu, Ni, Fe, Ge element in zinc sulfate
It can simultaneously be removed, reduce the content of impurity element in zinc sulfate, improve the purity of zinc sulfate；And also cause purification
Process can be completed in the environment of 55-80 DEG C, reduce the energy consumption of purification process；
(2) cobalt content is down to below 0.3mg/L by the present invention by 60~90mg/L, to meet to be electrolysed for 24 hours, 48 hours
It is required that；
(3) by addition except cobalt agent is significantly improved except cobalt impurity elimination effect, during thorough solution Purification of zinc sulfate solution
The excessive problem of zinc powder, the usage amount of zinc powder is not only reduced, improve the utilization rate of zinc powder, while it is molten to also improve zinc sulfate
The stability of liquid depuration quality, remarkable in economical benefits is simple to operate, practical；
(4) cleaned filtrate is accurately filtered with Sean filter in time, a small amount of filter slag is removed, from root
The cadmium metal eliminated in filter residue is dissolved into filtrate, ensures that purification filtering solution can meet the quality of new liquid for a long time
Standard requirement；
(5) technological process of zinc sulfate purification method of the invention is short, and purification cycle is short, and energy consumption is low, the amount of reagent of addition
Less, cost is relatively low, and production efficiency is high；And it will not also cause environment pollution, there is significant economic benefit and environmentally friendly valency
Value.
Embodiment
The present invention is further described below with reference to specific embodiment.
Embodiment 1
A kind of Technology for removing cobalt of high-cobalt zinc sulfate solution, comprises the following steps：
(1) at normal temperatures, supernatant solution in zinc sulfate is accurately filtered using Sean filter, after making accurate filtering
Solution solids suspension content be less than 50mg/L；
(2) by the middle supernatant solution after filtering, under the conditions of 70-80 DEG C, zincification powder 2.0-2.5Kg/m3, stirring reaction
0.5-1.0h, press filtration, obtain a net rear liquid；
(3) by one it is net after liquid temperature adjusting to 55-65 DEG C, be continuously added into zinc powder, stirring reaction 0.5-1.0h, press filtration, directly
Into solution, each primary metal ion concentration reaches Zn 120-150g/L, Cd 1-50mg/L, Cu 0.01-0.3mg/L, Ni
0.1-1.5mg/L, Fe 1.0-2.0mg/L, Ge 0.01-0.02mg/L, stop adding zinc powder, obtain two net rear liquid, and determine it
In cobalt content, wherein the addition of zinc powder is between 1.0-1.5Kg/m3Between；
(4) prepare and remove cobalt agent-A, come by the content of cobalt content and other metal ions in the step (3) two liquid after net
Glycine addition is calculated, the calculation formula of glycine addition is：Glycine addition (mg/L)=Co concentration (mg/L)+
Fe concentration (mg/L) } × (5)+{ other concentration of metal ions (mg/L) × (3) }；The glycine industrial water of content will be determined
After being dissolved by solid-liquid=0.15, pH value is adjusted to 8.0-9.0, obtained except cobalt agent-A；
(5) prepare and remove cobalt agent-B, come by the content of cobalt content and other metal ions in the step (3) two liquid after net
Natrium nitrosum addition is calculated, the calculation formula of natrium nitrosum addition is：Natrium nitrosum addition (mg/L)={ Co concentration
(mg/L)+Fe concentration (mg/L) } × (3)；After the natrium nitrosum for determining content is dissolved with industrial water by solid-liquid=0.25,
Cobalt agent-B must be removed；
(6) preheat, two net rear liquid are preheated to 55-80 DEG C；
(7) by except cobalt agent-A and except cobalt agent-B is added in two after preheating net rear liquid, 2-5min is stirred；
(8) the net rear liquor pH value of gained two in the step (9) is adjusted to 2.5-5.0, and keeps solution temperature in 55-
80 DEG C, stirring reaction 1.0-2.0h；
(9) press filtration, obtains new liquid, and remaining concentration of cobalt ions≤0.3mg/L in new liquid, other metal ions meet electrode will
Ask.
It is worth noting that, the material that the step (10) is used for adjusting pH value is sulfuric acid, Zn system is electrolysed the useless of output
Any of electrolyte, acetic acid, nitric acid, phosphoric acid.
In the present embodiment, 4-6 of the glycine addition by surveying cobalt content in two net rear liquid in the step (3)
Times.
In the present embodiment, the natrium nitrosum addition is by surveying cobalt content in two net rear liquid in the step (3)
1-2 times.
In addition, a kind of cobalt agent that removes of high-cobalt zinc sulfate solution is except cobalt agent-A and the step (7) in the step (5)
In except cobalt agent-B mixture.
Embodiment 2
A kind of high-cobalt zinc sulfate solution removes cobalt agent with embodiment 1, except that, a kind of high-cobalt zinc sulfate solution removes
Cobalt technique, comprises the following steps：
(1) at normal temperatures, supernatant solution in zinc sulfate is accurately filtered using Sean filter, after making accurate filtering
Solution solids suspension content be less than 50mg/L；
(2) by the middle supernatant solution after filtering, under the conditions of 70-80 DEG C, zincification powder 2.0-2.5Kg/m3, stirring reaction
0.5-1.0h, press filtration, obtain a net rear liquid；
(3) by one it is net after liquid temperature adjusting to 55-65 DEG C, be continuously added into zinc powder, stirring reaction 0.5-1.0h, press filtration, directly
Into solution, each primary metal ion concentration reaches Zn 120-150g/L, Cd 1-50mg/L, Cu 0.01-0.3mg/L, Ni
0.1-1.5mg/L, Fe 1.0-2.0mg/L, Ge 0.01-0.02mg/L, stop adding zinc powder, obtain two net rear liquid, and determine it
In cobalt content, wherein the addition of zinc powder is between 1.0-1.5Kg/m3Between；
(4) prepare and remove cobalt agent-A, come by the content of cobalt content and other metal ions in the step (3) two liquid after net
Glycine addition is calculated, the calculation formula of glycine addition is：Glycine addition (mg/L)=Co concentration (mg/L)+
Fe concentration (mg/L) } × (4)+{ other concentration of metal ions (mg/L) × (2) }；The sweet of content will be determined in the step (4)
After propylhomoserin is dissolved with industrial water by solid-liquid=0.1, pH value is adjusted to 8.0-9.0, obtained except cobalt agent-A；
(5) prepare and remove cobalt agent-B, come by the content of cobalt content and other metal ions in the step (3) two liquid after net
Natrium nitrosum addition is calculated, the calculation formula of natrium nitrosum addition is：Natrium nitrosum addition (mg/L)={ Co concentration
(mg/L)+Fe concentration (mg/L) } × (4)；After the natrium nitrosum for determining content is dissolved with industrial water by solid-liquid=0.3, obtain
Except cobalt agent-B；
(6) two net rear liquid are preheated to 55-80 DEG C；
(7) by except cobalt agent-A and except cobalt agent-B is added in two after preheating net rear liquid, 2-5min is stirred；
(8) the net rear liquor pH value of gained two in the step (9) is adjusted to 2.5-5.0, and keeps solution temperature in 55-
80 DEG C, stirring reaction 1.0-2.0h；
(9) press filtration, obtains new liquid, and remaining concentration of cobalt ions≤0.3mg/L in new liquid, other metal ions meet electrode will
Ask.
It is worth noting that, the material that the step (10) is used for adjusting pH value is sulfuric acid, Zn system is electrolysed the useless of output
Any of electrolyte, acetic acid, nitric acid, phosphoric acid.
In the present embodiment, 4-6 of the glycine addition by surveying cobalt content in two net rear liquid in the step (3)
Times.
In addition, the natrium nitrosum addition is by middle survey cobalt content in two net rear liquid 1-2 times of the step (3).
Embodiment 3
A kind of high-cobalt zinc sulfate solution removes cobalt agent with embodiment 1, except that, a kind of high-cobalt zinc sulfate solution removes
Cobalt technique, comprises the following steps：
(1) at normal temperatures, supernatant solution in zinc sulfate is accurately filtered using Sean filter, after making accurate filtering
Solution solids suspension content be less than 50mg/L；
(2) by the middle supernatant solution after filtering, under the conditions of 70-80 DEG C, zincification powder 2.0-2.5Kg/m3, stirring reaction
0.5-1.0h, press filtration, obtain a net rear liquid；
(3) by one it is net after liquid temperature adjusting to 55-65 DEG C, be continuously added into zinc powder, stirring reaction 0.5-1.0h, press filtration, directly
Into solution, each primary metal ion concentration reaches Zn 120-150g/L, Cd 1-50mg/L, Cu 0.01-0.3mg/L, Ni
0.1-1.5mg/L, Fe 1.0-2.0mg/L, Ge 0.01-0.02mg/L, stop adding zinc powder, obtain two net rear liquid, and determine it
In cobalt content, wherein the addition of zinc powder is between 1.0-1.5Kg/m3Between；
(4) prepare and remove cobalt agent-A, come by the content of cobalt content and other metal ions in the step (3) two liquid after net
Glycine addition is calculated, the calculation formula of glycine addition is：Glycine addition (mg/L)=Co concentration (mg/L)+
Fe concentration (mg/L) } × (6)+{ other concentration of metal ions (mg/L) × (4) }；The glycine industrial water of content will be determined
After being dissolved by solid-liquid=0.2, pH value is adjusted to 8.0-9.0, obtained except cobalt agent-A；
(5) prepare and remove cobalt agent-B, come by the content of cobalt content and other metal ions in the step (3) two liquid after net
Natrium nitrosum addition is calculated, the calculation formula of natrium nitrosum addition is：Natrium nitrosum addition (mg/L)={ Co concentration
(mg/L)+Fe concentration (mg/L) } × (2)；After the natrium nitrosum for determining content is dissolved with industrial water by solid-liquid=0.2, obtain
Except cobalt agent-B；
(6) preheat, two net rear liquid are preheated to 55-80 DEG C；
(7) by except cobalt agent-A and except cobalt agent-B is added in two after preheating net rear liquid, 2-5min is stirred；
(8) the net rear liquor pH value of gained two in the step (9) is adjusted to 2.5-5.0, and keeps solution temperature in 55-
80 DEG C, stirring reaction 1.0-2.0h；
(9) press filtration, obtains new liquid, and remaining concentration of cobalt ions≤0.3mg/L in new liquid, other metal ions meet electrode will
Ask.
It is worth noting that, the material that the step (10) is used for adjusting pH value is sulfuric acid, Zn system is electrolysed the useless of output
Any of electrolyte, acetic acid, nitric acid, phosphoric acid.
In the present embodiment, 4-6 of the glycine addition by surveying cobalt content in two net rear liquid in the step (3)
Times.
In addition, the natrium nitrosum addition is by middle survey cobalt content in two net rear liquid 1-2 times of the step (3).
Schematically the present invention and embodiments thereof are described above, the description is not restricted.So if
One of ordinary skill in the art is enlightened by it, without departing from the spirit of the invention, without the design of creativeness
Go out the frame mode similar to the technical scheme and embodiment, protection scope of the present invention all should be belonged to.
Claims (9)
1. a kind of Technology for removing cobalt of high-cobalt zinc sulfate solution, it is characterised in that comprise the following steps：
(1) at normal temperatures, supernatant solution in zinc sulfate is accurately filtered using Sean filter, made molten after accurate filtering
Liquid solid suspension content is less than 50mg/L；
(2) by the middle supernatant solution after filtering, under the conditions of 70-80 DEG C, zincification powder 2.0-2.5Kg/m3, stirring reaction 0.5-
1.0h, press filtration, obtain a net rear liquid；
(3) a net rear liquid temperature adjusting is continuously added into zinc powder, stirring reaction 0.5-1.0h, press filtration, Zhi Daorong to 55-65 DEG C
Each primary metal ion concentration reaches finite concentration in liquid, stops adding zinc powder, obtains two net rear liquid, and determine cobalt therein and contain
Amount；
(4) glycine addition is calculated by the content of cobalt content and other metal ions in the step (3) two net rear liquid；
(5) after the glycine that content is determined in the step (4) is dissolved with industrial water by solid-liquid=0.1-0.2, by pH value
8.0-9.0 is adjusted to, is obtained except cobalt agent-A；
(6) added by the content of cobalt content and other metal ions in the step (3) two liquid after net to calculate natrium nitrosum
Amount；
(7) after the natrium nitrosum that content is determined in the step (6) is dissolved with industrial water by solid-liquid=0.2-0.3, must remove
Cobalt agent-B；
(8) two net rear liquid are preheated to 55-80 DEG C；
(9) by except cobalt agent-A and except cobalt agent-B is added in two after preheating net rear liquid, 2-5min is stirred；
(10) the net rear liquor pH value of gained two in the step (9) is adjusted to 2.5-5.0, and keeps solution temperature in 55-80
DEG C, stirring reaction 1.0-2.0h；
(11) press filtration, obtains new liquid, and remaining concentration of cobalt ions≤0.3mg/L, other metal ions meet electrode requirement in new liquid.
A kind of 2. Technology for removing cobalt of high-cobalt zinc sulfate solution according to claim 1, it is characterised in that the step (3)
When the concentration that each primary metal ion reaches is in solution：Zn 120-150g/L, Cd 1-50mg/L, Cu 0.01-0.3mg/L,
Ni 0.1-1.5mg/L, Fe 1.0-2.0mg/L, Ge 0.01-0.02mg/L, stop adding zinc powder.
A kind of 3. Technology for removing cobalt of high-cobalt zinc sulfate solution according to claim 1 or 2, it is characterised in that the step
(3) addition of zinc powder is between 1.0-1.5Kg/m3Between.
A kind of 4. Technology for removing cobalt of high-cobalt zinc sulfate solution according to claim 1, it is characterised in that the step (4)
The calculation formula of middle glycine addition is：Glycine addition mg/L={ Co concentration mg/L+Fe concentration mg/L } × (4-6)+
{ other concentration of metal ions mg/L × (2-4) }.
A kind of 5. Technology for removing cobalt of high-cobalt zinc sulfate solution according to claim 1 or 2, it is characterised in that the step
(6) calculation formula of Sodium Nitrite addition is：Natrium nitrosum addition mg/L={ Co concentration mg/L+Fe concentration mg/L } ×
(2-4)。
A kind of 6. Technology for removing cobalt of high-cobalt zinc sulfate solution according to claim 1, it is characterised in that the step (10)
For adjusting the material of pH value as any of sulfuric acid, the waste electrolyte of Zn system electrolysis output, acetic acid, nitric acid, phosphoric acid.
A kind of 7. Technology for removing cobalt of high-cobalt zinc sulfate solution according to claim 1 or 4, it is characterised in that the sweet ammonia
Sour addition is by middle survey cobalt content in two net rear liquid 4-6 times of the step (3).
A kind of 8. Technology for removing cobalt of high-cobalt zinc sulfate solution according to claim 1, it is characterised in that the natrium nitrosum
Addition is by middle survey cobalt content in two net rear liquid 1-2 times of the step (3).
9. a kind of high-cobalt zinc sulfate solution Technology for removing cobalt implemented described in claim 1 removes cobalt agent, it is characterised in that described to remove
Cobalt agent be in the step (5) except in cobalt agent-A and the step (7) except cobalt agent-B mixture.
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| CN114058872A (en) * | 2021-11-24 | 2022-02-18 | 白银有色集团股份有限公司 | Method for improving grade of cobalt slag of zinc hydrometallurgy |
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|---|---|---|---|---|
| CN1310240A (en) * | 2000-02-25 | 2001-08-29 | 中南工业大学 | Method of utilizing beta-naphthol for eliminating Co in main and subsidiary zinc electrolyzing systems |
| CN103194600A (en) * | 2013-04-23 | 2013-07-10 | 吴鋆 | Method for purifying zinc sulfide solution |
| CN103468952A (en) * | 2013-09-22 | 2013-12-25 | 云南永昌铅锌股份有限公司 | Method for treating zinc sulfate solution |
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